CN107188567B - Preparation method of aluminum nitride ceramic with high thermal conductivity - Google Patents
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Abstract
A preparation method of aluminum nitride ceramics with high thermal conductivity belongs to the technical field of aluminum nitride ceramics preparation. Taking aluminum nitride powder as a main raw material and absolute ethyl alcohol as a solventIntroducing 2-6 wt% of ternary sintering aid, performing wet ball milling, drying, granulating, dry pressing, cold isostatic pressing, degreasing and sintering to obtain the high-thermal-conductivity aluminum nitride ceramic, wherein the thermal conductivity of the aluminum nitride ceramic is 180-230 W.m‑1·K‑1The density is more than or equal to 99.3 percent. The method has the advantages that the prepared aluminum nitride ceramic has a uniform microstructure; the preparation process is simple and convenient for batch production. The introduced ternary sintering aid can well regulate and control the structural performance of the aluminum nitride ceramic, so that the preparation of the aluminum nitride ceramic with high thermal conductivity through pressureless sintering is realized.
Description
Technical Field
The invention belongs to the technical field of aluminum nitride ceramic preparation, and relates to a preparation method of aluminum nitride ceramic with high thermal conductivity.
Background
The aluminum nitride ceramic has excellent heat conducting performance, electric insulating performance, high temperature resistance, low dielectric constant, linear expansion coefficient matched with that of silicon, no toxicity and other features, and thus may be used as ideal basic material and electronic device packing material.
High thermal conductivity is an advantage for industrial applications of aluminum nitride ceramics. To achieve the preparation of high thermal conductivity ceramics, two conditions must be met: firstly, the aluminum nitride ceramic has higher compactness; secondly, the solid solution oxygen content in the aluminum nitride ceramic crystal lattice is required to be as low as possible. In practical production, a sintering aid such as rare earth compounds (yttrium oxide, samarium oxide, dysprosium oxide, yttrium fluoride, samarium fluoride and the like) or alkaline earth metal compounds (calcium oxide, boron oxide, calcium fluoride and the like) is generally introduced, and reacts with alumina at a high temperature to generate a second phase so as to reduce the content of solid solution oxygen in crystal lattices and promote sintering, thereby realizing the preparation of the aluminum nitride ceramic with high thermal conductivity. Chinese patent (CN102030538B) discloses a method for preparing aluminum nitride ceramics and the aluminum nitride ceramics prepared by the method, wherein one or more of yttrium oxide, calcium fluoride and dysprosium oxide are used as sintering aids to prepare a series of aluminum nitride ceramicsWherein the thermal conductivity of the aluminum nitride ceramic prepared by using yttrium oxide and calcium oxide as the composite sintering aid is the highest (180 W.m)-1·K-1). Tohru et al (script materials, 2005,52:583--1·K-1The aluminum nitride ceramic of (1). YU et al (Journal of the European Ceramic Society,2002,22:247--1·K-1The aluminum nitride ceramic of (1). It can be seen that the thermal conductivity of aluminum nitride ceramics has a very important relationship with the choice of sintering aid. Therefore, the search and development of the multi-component system sintering aid suitable for the aluminum nitride ceramic are important for the preparation of the aluminum nitride ceramic with high thermal conductivity.
Disclosure of Invention
The invention aims to provide a ternary sintering aid (cerium oxide, one of other rare earth compounds and one of alkaline earth metal compounds) for preparing aluminum nitride ceramics and a preparation method thereof, which can realize the pressureless sintering preparation of the aluminum nitride ceramics with high thermal conductivity. Under the same condition, the performance of the aluminum nitride ceramic prepared by introducing the ternary sintering aid is superior to the performance of the aluminum nitride ceramic prepared by introducing the single and binary composite sintering aids.
The technical scheme of the invention is as follows: a preparation method of high-thermal-conductivity aluminum nitride ceramic comprises the following steps:
1) preparing materials: weighing aluminum nitride powder and a sintering aid in proportion, placing the mixture into a ball milling tank, adding absolute ethyl alcohol and zirconia milling balls, and performing ball milling to obtain uniformly mixed slurry, wherein the ball milling speed is 150-180 r/min;
2) molding: and (3) putting the slurry into a low-temperature oven at 50-70 ℃, drying, grinding, crushing, adding a proper amount of binder, uniformly mixing, and sieving the powder. Putting the powder into a steel mould, carrying out primary forming on the powder on a press machine, then placing the formed green body into a cold isostatic press after plastic packaging, and carrying out secondary pressure forming to finally obtain an aluminum nitride ceramic green body;
3) degreasing: placing the aluminum nitride green body in a muffle furnace, and degreasing the aluminum nitride green body in an air atmosphere;
4) and (3) sintering: and (3) placing the degreased green body in a high-temperature sintering furnace, and sintering the sample at 1800-1900 ℃ in a nitrogen atmosphere, wherein the heat preservation time is 2-6 h. And after sintering, cooling to 1600-1700 ℃ at a cooling rate of 1-5 ℃/min, and then cooling to room temperature along with the furnace to obtain the aluminum nitride ceramic.
Preferably, the sintering aid in step (1) is a ternary composite sintering aid, which contains cerium oxide, one of rare earth compounds of yttrium oxide, samarium oxide, dysprosium oxide, yttrium fluoride, samarium fluoride and the like, and one of alkaline earth metal compounds of calcium oxide, boron oxide, calcium fluoride and the like. Wherein the introduced mass of the cerium oxide, other rare earth compounds and alkaline earth metal compounds respectively accounts for 0.5-1.5%, 1-3% and 0.5-1.5% of the total mass of the powder;
preferably, in the burdening process in the step (1), in order to realize rapid and uniform mixing of the ceramic powder, the mass ratio of the ceramic powder to the grinding balls to the absolute ethyl alcohol is 1:1: 1-1: 2: 3;
preferably, in order to ensure the uniformity of the structure of the formed blank in the forming process in the step (2), the forming process is as follows: the one-step forming pressure is 20-40 MPa, and the pressure maintaining time is 1-3 min; in the secondary forming process, maintaining the pressure at 80-120 MPa for 1-6min, and maintaining the pressure at 200-240 MPa for 1-6 min; the pressure increasing and reducing speed is within the range of 10-20 MPa/min;
preferably, the degreasing process in the step (3) must ensure that defects such as cracks cannot be generated in the blank during degreasing, so as to ensure the uniformity of the microstructure of the subsequent sintered sample; in view of the above consideration, the degreasing temperature range of the blank is generally 450-600 ℃, the heating rate is less than or equal to 4 ℃/min, and the heat preservation time is 2-6 h;
preferably, the sintering process in step (4) must ensure the densification and sintering of the green body, and simultaneously avoid the occurrence of bending deformation and the like in the sintering process, wherein the sintering temperature is generally controlled to be 1800-1900 ℃, and the heating rate is less than or equal to 8 ℃/min, keeping the temperature for 2-6 h; and after the heat preservation is finished, firstly, controlling the temperature to be 1600-1700 ℃, cooling at the rate of 1-5 ℃/min, and then cooling to the room temperature along with the furnace. The thermal conductivity of the obtained aluminum nitride ceramic is 180-230 W.m-1·K-1The density is more than or equal to 99.3 percent.
The invention has the advantages that the thermal conductivity of the obtained aluminum nitride ceramic is 180-230 W.m-1·K-1The density is more than or equal to 99.3 percent. The microstructure of the prepared aluminum nitride ceramic is uniform; the preparation process is simple and convenient for batch production. The introduced ternary sintering aid can well regulate and control the structural performance of the aluminum nitride ceramic, so that the preparation of the aluminum nitride ceramic with high thermal conductivity through pressureless sintering is realized.
Drawings
FIG. 1 is a microscopic structure of high thermal conductivity aluminum nitride ceramic.
Detailed Description
1, accurately weighing aluminum nitride powder, samarium oxide, cerium oxide and calcium fluoride powder in sequence according to the mass ratio of 96:2.5:1:0.5, placing the powder in a nylon ball milling tank, simultaneously adding stearic acid with the mass ratio of 0.3% as a dispersing agent, adding absolute ethyl alcohol and zirconia balls as ball milling media, and carrying out wet ball milling for 4 hours. Wherein the mass ratio of the powder material to the absolute ethyl alcohol to the zirconia balls is 1:1:2, and the ball milling speed is 160 r/min. Drying the slurry to obtain a uniformly mixed material;
2 adding polyvinyl butyral solution as a binder, uniformly mixing with the mixed material, screening by a 80-mesh screen, putting the powder into a steel mould, and pressing on a press machine to form a green body, wherein the forming pressure is 40 MPa; then packaging the green body in a plastic package way, and placing the green body in a cold isostatic press for secondary pressing, wherein the pressure for pressing and molding is 100MPa, the pressure is maintained for 60s, and the pressure maintaining time at 220MPa is 180 s;
3, placing the molded green body in a degreasing furnace to carry out glue removal in air atmosphere. The heating rate is 2 ℃/min, the glue temperature is 500 ℃, and the heat preservation time is 4 h;
4, placing the degreased green body into a crucible, placing the crucible in a high-temperature sintering furnace for sintering in a nitrogen atmosphere, heating to 1860 ℃ at a certain speed, keeping the temperature for 4 hours, cooling to 1700 ℃ at a certain speed after sintering, and cooling to room temperature along with the furnace to obtain a high-thermal-conductivity aluminum nitride ceramic sample;
the aluminum nitride ceramic sample prepared by the process has compact microstructure (shown in figure 1), and volume density of 3.3g/cm3The porosity is 0.6%, the density is 99.4%, and the thermal conductivity is 201.3 W.K-1·m-1Compared with the aluminum nitride ceramic sample prepared by single (4 wt% of samarium oxide) and binary sintering aids (3 wt% of samarium oxide-1 wt% of cerium oxide; 3.5 wt% of samarium oxide-0.5 wt% of calcium fluoride) under the same condition, the thermal conductivity of the aluminum nitride ceramic sample is high.
Claims (4)
1. A preparation method of aluminum nitride ceramic with high thermal conductivity is characterized by comprising the following steps:
1) preparing materials: weighing aluminum nitride powder and a ternary sintering aid consisting of 0.5-1% of cerium oxide, 1-2.5% of other rare earth compounds and 0.5-1.5% of alkaline earth metal compounds according to the weight percentage, and then preparing and obtaining uniformly mixed slurry by adopting a wet mixing process, wherein a liquid medium for wet mixing is absolute ethyl alcohol, and the ball milling rotating speed is 150-180 r/min;
the other rare earth compound in the ternary sintering aid is one of yttrium oxide, samarium oxide, dysprosium oxide, yttrium fluoride and samarium fluoride; the alkaline earth metal compound is calcium fluoride;
2) molding: drying the slurry obtained in the step 1) in a low-temperature oven at 50-70 ℃, adding a binder for granulation, sieving, dry-pressing, and then performing a step-by-step pressurizing isostatic pressing process to obtain a green body;
3) degreasing: placing the green body obtained in the step 2) in a muffle furnace, and preserving heat for 2-6 h at 450-600 ℃;
4) and (3) sintering: placing the green body subjected to the heat treatment in the step 3) in a high-temperature sintering furnace, and preserving heat for 2-4 hours at 1860-1900 ℃ in a nitrogen atmosphere; after sintering, controlling the temperature to reduce to 1600-1700 ℃, reducing the temperature at the rate of 1-5 ℃/min, and then cooling to room temperature along with the furnace to obtain aluminum nitride ceramic; the thermal conductivity of the aluminum nitride ceramic prepared by the process is 180-220 W.m-1·K-1The density is more than or equal to 99.3 percent.
2. The method according to claim 1, wherein the mass ratio of the sintering aid in step 1) is relative to the mixed powder, and the mixed powder is a mixture of a ternary sintering aid and aluminum nitride powder.
3. The method as claimed in claim 1, wherein the binder used in step 2) includes but is not limited to paraffin wax and polyvinyl butyral organic binder, and the mass ratio of the binder to be introduced is 1-3% of the mass of the mixed powder.
4. The method of claim 1, wherein the parameters of the step pressure cold isostatic pressing process used in step 2) are: maintaining the pressure for 1-6min at 80-120 MPa and for 1-6min at 200-240 MPa, wherein the pressure increasing and reducing rates are both within the range of 10-20 MPa/min.
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| CN109761617B (en) * | 2019-02-22 | 2021-11-05 | 福建臻璟新材料科技有限公司 | F-Ca-Lu doped aluminum nitride complex phase ceramic green body and preparation process thereof |
| CN109761618A (en) * | 2019-03-15 | 2019-05-17 | 西安航空学院 | A kind of high-densit boron carbide enhancing Aluminum nitride composite ceramic preparation method |
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| CN115784750A (en) * | 2022-12-13 | 2023-03-14 | 航天特种材料及工艺技术研究所 | High-density aluminum nitride ceramic and preparation method thereof |
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| CN1130607A (en) * | 1995-11-17 | 1996-09-11 | 清华大学 | Method for manufacturing high-heat conductivity aluminium nitride ceramics |
| CN101638319B (en) * | 2008-07-29 | 2012-12-12 | 比亚迪股份有限公司 | Aluminum nitride composite material preparation method |
| CN105948759A (en) * | 2016-06-08 | 2016-09-21 | 山东鹏程陶瓷新材料科技有限公司 | Aluminum nitride ceramic substrate prepared by vacuum hot-pressing sintering method and preparation method thereof |
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